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CN106537660B - Lithium-sulfur battery - Google Patents

Lithium-sulfur battery Download PDF

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CN106537660B
CN106537660B CN201580029063.2A CN201580029063A CN106537660B CN 106537660 B CN106537660 B CN 106537660B CN 201580029063 A CN201580029063 A CN 201580029063A CN 106537660 B CN106537660 B CN 106537660B
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lithium
sulfur
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electrolyte
dinitrile
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CN106537660A (en
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塞巴斯蒂安·德西拉尼
阿什利·库克
格雷戈里·施密特
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Gelion Technologies Pty Ltd
Arkema France SA
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Oxis Energy Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
    • H01M10/0566—Liquid materials
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    • H—ELECTRICITY
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    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/381—Alkaline or alkaline earth metals elements
    • H01M4/382—Lithium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • H01M4/5815—Sulfides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0017—Non-aqueous electrolytes
    • H01M2300/0025—Organic electrolyte
    • H01M2300/0028—Organic electrolyte characterised by the solvent
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/409—Separators, membranes or diaphragms characterised by the material
    • H01M50/411—Organic material
    • H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
    • H01M50/417—Polyolefins
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/409—Separators, membranes or diaphragms characterised by the material
    • H01M50/411—Organic material
    • H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
    • H01M50/423—Polyamide resins
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
    • H01M50/491—Porosity
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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Abstract

The present invention relates to a lithium-sulfur battery comprising: an anode comprising lithium metal or a lithium metal alloy; a cathode containing a mixture of an electroactive sulfur material and a solid conductive material; and a liquid electrolyte comprising at least one lithium salt and a dinitrile-containing solvent.

Description

Lithium-sulfur battery
Technical Field
The present invention relates to a lithium-sulfur battery.
Background
A typical lithium sulfur battery includes an anode (negative electrode) formed of lithium metal or lithium metal alloy and a cathode (positive electrode) formed of elemental sulfur or other electroactive sulfur material. Sulfur or other electroactive sulfur-containing materials may be mixed with conductive materials (e.g., carbon) to improve their conductivity. Typically, the carbon and sulfur are milled and then mixed with a solvent and a binder to form a slurry. The slurry is coated on a current collector and then dried to remove the solvent. The resulting structure is calendered to form a composite structure that is cut into a desired shape to form the cathode. A separator was placed on the cathode, and a lithium anode was placed on the separator. An electrolyte is introduced into the cell to wet the cathode and separator. The electrolyte typically includes an electrolyte salt dissolved in a solvent.
The lithium sulfur battery is a secondary battery, and can be recharged by applying an external current to the battery. Such rechargeable batteries have a potentially wide range of applications. Important considerations in the development of lithium-sulfur secondary batteries include gravimetric energy, cycle life, and ease of battery assembly.
When a lithium sulfur battery is discharged, sulfur in the cathode is reduced in two stages. In a first stage, an electroactive sulfur material (e.g., elemental sulfur) is reduced to a polysulfide species, Sn 2-(n.gtoreq.2), these substances are usually dissolved in the electrolyte. In the second stage of discharge, the polysulphide species are reduced to lithium sulphide, Li2S, lithium sulfide is insoluble. When the battery is charged, the two-stage mechanism occurs in reverse, with the lithium sulfide being oxidized to lithium polysulfide and then to lithium and sulfur.
In addition to suitable solvents as electrolyte salts, the solvents used in lithium sulfur batteries should not react with the lithium metal anode and act as good solvents for the polysulfide species formed upon discharge. Thus, the solvent requirements of lithium-sulfur batteries are significantly more complex than those of lithium-ion batteries due to the multi-dimensionality introduced at least in part by the intermediate species formed during charging and discharging of the lithium-sulfur batteries. Many of the solvents (e.g., carbonates) typically used in lithium ion batteries are not suitable for use in lithium-sulfur batteries because they react with polysulfides formed upon discharge, particularly at high sulfur loadings. Therefore, the performance of the electrolyte solvent in a lithium-sulfur battery cannot be predicted from its performance as an electrolyte solvent in a lithium-ion battery.
Disclosure of Invention
Before describing particular embodiments of the present invention, it is to be understood that this invention is not limited to the particular batteries, methods, or materials disclosed herein. It is also to be understood that the terminology used herein is used for the purpose of describing particular examples only, and is not intended to be limiting, since the scope of protection will be defined by the claims and equivalents thereof.
In describing and claiming the battery and method of the present invention, the following terminology will be used: the singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. Thus, for example, reference to "an anode" includes reference to one or more of such elements.
According to an aspect of the present invention, there is provided a lithium sulfur battery including:
an anode comprising lithium metal or a lithium metal alloy;
a cathode containing a mixture of an electroactive sulfur material and a solid conductive material; and
a liquid electrolyte comprising at least one lithium salt and a dinitrile-containing solvent.
In embodiments of the present invention, it has been found that the gravimetric energy of lithium sulfur batteries can be increased by using dinitriles as electrolyte solvents. It has also been found that electrolytes formed using dinitriles as solvents can also have advantageous viscosity characteristics. Thus, such an electrolyte can be applied to the cathode in a convenient and efficient manner, facilitating efficient and convenient assembly of the battery. In embodiments of the present invention, it has also been found that the cycle life of lithium sulfur batteries can also be increased by using dinitriles as solvents in the lithium sulfur batteries.
In embodiments of the present invention, it has also been found that dinitriles can be used as solvents to improve the low temperature performance of lithium sulfur batteries. For example, in certain embodiments, the electrolyte may remain in liquid form at temperatures below 0 ℃, such as below-10 ℃ (e.g., up to-30 ℃).
The dinitrile may have formula (I):
Figure BDA0001167595660000021
wherein:
n is an integer of 2 to 10, and
at each-CR1R2In the bond, R1And R2Each independently selected from H, -OH, amine, amide, ether and C1To C6An alkyl group.
For the avoidance of doubt, each-CR1R2The bonds may be the same or different. In one embodiment, -CR1R2One of the bonds being different from-CR in a dinitrile1R2-the rest of the bond. Andthe remainder being-CR1R2-CR having different-bonds1R2The bond may be present in the vicinity of the CN group.
When R is1And/or R2When an amine, the amine may have the formula-NRaRbWherein R isaAnd RbEach independently is H or a hydrocarbyl group. Suitable hydrocarbyl groups include alkyl groups, e.g. C1-C4Alkyl (e.g., methyl, ethyl, propyl, or butyl). For example, -NRaRbMay be-NH2or-N (CH)3)2. The amine may be a primary, secondary or tertiary amine group.
When R is1And/or R2When an amide, the amide may be-NRaC(O)RbWherein R isaAnd RbEach independently is H or a hydrocarbyl group. Suitable hydrocarbyl groups include alkyl groups, e.g. C1To C4Alkyl (e.g., methyl, ethyl, propyl, or butyl). For example, -NRaC(O)RbCan be-NHC (O) CH3。
When R is1And/or R2When an ether group, the ether may have the formula-ORcWherein R iscIs a hydrocarbyl group. Suitable hydrocarbyl groups include alkyl groups, e.g. C1To C4Alkyl (e.g., methyl, ethyl, propyl, or butyl). For example, -ORcThe group may be-OCH3。
When R is1And/or R2When an alkyl group, the alkyl group may be C1To C6Alkyl radicals, such as the methyl, ethyl, propyl, isopropyl, n-butyl, isobutyl and tert-butyl, pentyl or hexyl radical.
In one embodiment, the dinitrile of formula (I) comprises a compound having at least 2, e.g., 2 to 4-CR1R2-a bond (represented by the formula-CH)2-composition). Optionally, the dinitrile of formula (I) may also include a dinitrile of formula-CHR2One or two of-CR1R2-a bond. -CHR2The-bond may be adjacent to the-CN group.
In one embodiment, the dinitrile has formula (II):
Figure BDA0001167595660000031
wherein:
p is 0 or 1, and p is,
q is an integer of 1 to 9,
r is 0 or 1, and
R3、R4、R5and R6Each independently selected from H and C1To C6Alkyl (e.g., methyl, ethyl, propyl, isopropyl, n-butyl, isobutyl, and tert-butyl, pentyl, or hexyl, preferably methyl).
Preferably, R3And R4At least one of which is H, and R5And R6At least one of which is H. Preferably, R3、R4、R5And R6At least one of them being C1To C6An alkyl group. In one embodiment, R3Is H; r5Is H; and R is4And R6At least one of them being C1To C6An alkyl group. For example, in one embodiment, R3Is H; r5Is H; r4Is H and R6Is C1To C6An alkyl group.
In one embodiment, p is 0 and r is 1. In one embodiment, q is 2. For example, p may be 0, r may be 1, and q may be 2.
Examples of suitable dinitriles include 2-methylglutaronitrile, succinonitrile and adiponitrile.
As described above, the electrolyte further includes a lithium salt. Suitable lithium salts include lithium hexafluorophosphate (LiPF)6) Lithium hexafluoroarsenate (LiAsF)6) Lithium perchlorate (LiClO)4) Lithium trifluoromethanesulfonylimide (LiN (CF)3SO2)2) Lithium fluoroborate (LiBF)4) Lithium trifluoromethanesulfonate (CF)3SO3Li) and lithium bis (oxalato) borate (LiB (C)2O4)2) At least one of (1). Preferably, the lithium salt is lithium trifluoromethanesulfonylimide (LiN (CF)3SO2)2))。
The concentration of the lithium salt in the electrolyte is preferably 0.1 to 5M, more preferably 0.2 to 3M, for example 0.4 to 2M (e.g., 0.5 to 1M).
As described above, the lithium sulfur battery of the present invention includes an anode, a cathode, an electrolyte, and an optional porous separator. A porous separator may be positioned between the anode and the cathode. The anode is formed of lithium metal or a lithium metal alloy. Preferably, the anode is a metal foil electrode, such as a lithium foil electrode. The lithium foil is formed of lithium metal or a lithium metal alloy.
The cathode of the cell includes a mixture of an electroactive sulfur material and a conductive material. The mixture forms an electroactive layer, which can be placed in contact with a current collector.
Electroactive sulfur materials can include elemental sulfur, sulfur-based organic compounds, sulfur-based inorganic compounds, and sulfur-containing polymers. Preferably, elemental sulphur is used.
The solid conductive material may be any suitable conductive material. Preferably, the solid conductive material may be formed of carbon. Examples include carbon black, carbon fiber, graphene, and carbon nanotubes. Other suitable materials include metals (e.g., flakes, filings, and powders) and conductive polymers. Carbon black is preferably used.
The mixture of electroactive sulfur material and conductive material may be applied to the current collector in the form of a slurry in a solvent (e.g., water or an organic solvent). The solvent may then be removed and the resulting structure calendered to form a composite structure, which may be cut into a desired shape to form a cathode. A separator may be placed on the cathode and a lithium anode placed on the separator. An electrolyte may then be incorporated into the assembled cell to wet the cathode and separator.
Alternatively, the electrolyte may be coated on the cathode after the cathode is formed. A separator can then be placed on the coated cathode and an anode placed on the separator.
As noted above, electrolytes formed using dinitriles as solvents may also have favorable viscosity characteristics. Thus, such an electrolyte can be applied to the cathode in a convenient and efficient manner, facilitating efficient and convenient assembly of the battery. In a preferred embodiment of the invention, the electrolyte is incorporated into the battery assembly by coating the electrolyte on the cathode, placing the separator on the coated cathode and placing the anode on the separator. The coating may be performed in any suitable manner, for example, by spraying, extruding, vacuum filling, pouring and/or spreading the electrolyte on the active sulfur material. After the electrolyte is incorporated into the battery assembly, the battery can be sealed, for example, in a housing. The housing may be waterproof and/or airtight. Suitable housings include bags.
Where a separator is used, the separator may comprise any suitable porous substrate that allows ions to move between the electrodes of the cell. The separator should be located between the electrodes to prevent direct contact between the electrodes. The porosity of the substrate should be at least 30%, preferably at least 50%, e.g. above 60%. Preferably, the porosity of the separator is 40-60%, more preferably 45-55%, e.g. 50%. Suitable separators include webs formed from polymeric materials. Suitable polymers include polypropylene, nylon, and polyethylene. Non-woven polypropylene is particularly preferred. Multiple layers of separator may be used.
Preferably, the separator is selected from the group consisting of non-woven polypropylene and polyethylene.
Preferably, the permeability of the separator is less than 300Gurley, more preferably less than 250Gurley, for example 200 Gurley.
The lithium-sulfur battery of the present invention is a secondary battery. When a lithium sulfur battery is discharged, sulfur in the cathode is reduced in two stages. In a first stage, an electroactive sulfur material (e.g., elemental sulfur) is reduced to a polysulfide species, Sn 2-(n.gtoreq.2). These materials are typically dissolved in the electrolyte. In the second stage of discharge, the polysulphide species are reduced to lithium sulphide, Li2S, lithium sulfide is typically deposited on the surface of the anode.
When the battery is charged, the two-stage mechanism occurs in reverse, with the lithium sulfide being oxidized to lithium polysulfide and then to lithium and sulfur. Thus, the electrolyte of the cell may comprise polysulphides species dissolved in the dinitrile.
Detailed Description
Example 1
All electrolytes were prepared by dissolving bis (trifluoromethylsulfonyl) imide salt (LiTFSI) in the solvent listed in the following table at a concentration of 0.5M. The electrolyte was then stirred at 30 ℃ for 1 hour or until completely dissolved.
The electrolyte was then incorporated under dry chamber conditions (dew point)<-50 ℃) of the assembled cell. The cathode material consisted of sulfur, carbon black, and polyethylene oxide binder (PEO) in a ratio of 70:10:20(w/w), respectively. Casting the cathode material to a casting mold having a thickness of 1.9-2.0mAh/cm2Carbon coated aluminum foil of typical surface capacity. By using electrolyte (3.5 μ L/mAh/cm)2) The cathode was wetted and a polypropylene separator (Celgard 3501) and a 100 μm thick lithium foil anode were stacked in that order to assemble a cell.
The cell discharge-charge performance was evaluated in a constant current mode at 30 ℃ using a Maccor multichannel cycler with a voltage range of 1.5-2.45V. The cell was discharged and charged at current densities of 0.2C and 0.1C, respectively.
The following table shows the gravimetric energy density achieved for each cell. This was compared to a reference cell formed using 0.5M lithium bis (trifluoromethylsulfonyl) imide salt (LiTFSI) in sulfolane. As can be seen from the table, the cell formed using dinitrile as electrolyte solvent showed significantly improved gravimetric energy density compared to the reference cell and the cell formed using mononitrile as electrolyte solvent.
Figure BDA0001167595660000061
MPN ═ 3-methoxypropionitrile
MGN-2-methylglutaronitrile
Example 2
A lithium sulfur cell formed using lithium littdi (4, 5-dicyano-2- (trifluoromethyl) imidazolium) in 2-methylglutaronitrile as the electrolyte cycles over a temperature range of-10 ℃ to 30 ℃. The charge-discharge curves at various temperatures are shown in fig. 1. Comparative cells were formed using sulfolane as the electrolyte solvent. A comparative charge-discharge curve is shown in fig. 2. As can be seen from the figure, the battery formed using 2-MGN as an electrolyte solvent has excellent performance at low temperature.

Claims (9)

1. A lithium sulfur battery, comprising:
an anode comprising lithium metal or a lithium metal alloy;
a cathode containing a mixture of an electroactive sulfur material and a solid conductive material; and
a liquid electrolyte comprising at least one lithium salt, lithium polysulfide and a solvent comprising a dinitrile, wherein lithium polysulfide is dissolved in the dinitrile, the dinitrile having formula (II)
Figure FDA0002456340810000011
Wherein:
p is 0 or 1, and p is,
q is an integer of 1 to 9,
r is 0 or 1, and
R3、R4、R5and R6Each independently selected from H and C1To C6Alkyl, and wherein R3And R4At least one of which is H, and R5And R6At least one of which is H.
2. The battery of claim 1, wherein R is3、R4、R5And R6At least one of them being C1To C6An alkyl group.
3. The battery of claim 1, wherein p is 0 and r is 1.
4. The battery of claim 3, wherein q is 2.
5. The battery of claim 3, wherein R is5And R6At least one of which is H and the other is C1To C6An alkyl group.
6. The battery of claim 1, wherein C is1To C6The alkyl group is a methyl group.
7. The cell of claim 1, wherein the dinitrile is selected from at least one of 2-methylglutaronitrile, succinonitrile, and adiponitrile.
8. The cell of any one of claims 1 to 7, wherein the electroactive sulfur material comprises elemental sulfur.
9. The battery of any of claims 1-7, wherein the solid conductive material comprises carbon.
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